U.S. patent application number 10/433109 was filed with the patent office on 2004-06-03 for fibrillation of natural fibres.
Invention is credited to Russell, Stephen J..
Application Number | 20040103481 10/433109 |
Document ID | / |
Family ID | 9904680 |
Filed Date | 2004-06-03 |
United States Patent
Application |
20040103481 |
Kind Code |
A1 |
Russell, Stephen J. |
June 3, 2004 |
Fibrillation of natural fibres
Abstract
Fibrillation of certain cellulosic fibres has been widely
studied, and fibrillation can be utilised to improve fabric
performance, for example strength, absorbency, surface area
together with handle and opacity. However, it believed that
keratinous fibres such as wool have not been treated in this way.
The invention seeks to provide a fibrillated keratinous fibre
fabric and a method of fibrillating natural fibres. A textile
fabric of keratinous fibre is disclosed characterised by the
presence of fibrils, micro-fibrils and proto-fibrils. The fibrils
may be further characterised as having diameters in the range 3
.mu.m to 5 .mu.m and by having lengths in the range 25 .mu.m to 60
.mu.m. Preferably, the fabric is a woven, knitted, non-woven or
composite fabric. A method of treating natural fibres is also
disclosed which comprises:- a pre-treatment to remove surface lipid
materials or scales, e.g. using an oxidising agent; a treatment to
remove or partially remove intercellular cement, e.g. using an
enzyme; and the application of mechanical agitation under aqueous
conditions, e.g. hydroentanglement, to complete fibrillation.
Inventors: |
Russell, Stephen J.; (North
Yorkshire, GB) |
Correspondence
Address: |
Harold W Milton Jr
Howard & Howard Attorneys
The Pinehurst Office Center Suite 101
39400 Woodward Avenue
Bloomfield Hills
MI
48304-5151
US
|
Family ID: |
9904680 |
Appl. No.: |
10/433109 |
Filed: |
January 20, 2004 |
PCT Filed: |
December 5, 2001 |
PCT NO: |
PCT/GB01/05368 |
Current U.S.
Class: |
8/115.51 |
Current CPC
Class: |
D06M 13/364 20130101;
D06L 1/20 20130101; D06M 11/50 20130101; D06M 13/52 20130101; D06M
11/30 20130101; D06M 10/025 20130101; D06M 11/84 20130101; D06M
16/003 20130101; D06C 29/00 20130101; D06L 1/12 20130101; D06L 4/40
20170101; D06L 1/16 20130101 |
Class at
Publication: |
008/115.51 |
International
Class: |
D06M 010/00 |
Foreign Application Data
Date |
Code |
Application Number |
Dec 6, 2000 |
GB |
0029932.1 |
Claims
1. A textile fabric of keratinous fibres characterised by the
presence of fibrils, micro-fibrils and proto-fibrils.
2. A fabric as claimed in claim 1 wherein the fibrils are further
characterised as having diameters in the range 3 .mu.m to 5 .mu.m
and by having lengths in the range 25 .mu.m to 60 .mu.m.
3. A fabric as claimed in either of claims 1 or 2 wherein the
fabric is a woven, knitted, non-woven or composite fabric.
4. A method of treating natural fibres which comprises: a
pre-treatment to remove surface lipid materials or scales; a
treatment to remove or partially remove intercellular cement; and
the application of mechanical agitation to complete
fibrillation.
5. A method as claimed in claim 4 wherein the first step is carried
out with an oxidising agent.
6. A method as claimed in claim 5 wherein the oxidising agent is
permonosulphuric acid or its salt (PMS), dichloroisocyanuric Acid
or its salt (DCCA), or sodium hypochlorite.
7. A method as claimed in claim 4 or 5 wherein the first step is
carried out using electrical discharge (plasma) treatments.
8. A method as claimed in any of claims 4 to 7 wherein he second
stage of the process, namely removal of intercellular cement, is
carried out using an enzyme treatment.
9. A method as claimed in claim 8 wherein the enzyme is Papain.
10. A method as claimed in any of claims 4 to 9 wherein the
mechanical agitation is preferably carried out under aqueous
conditions.
11. A method as claimed in any of claims 4 to 10 wherein energy is
introduced by the process known as "hydroentanglement" in which
water jets are used to agitate the fibres and partially break them
down into smaller, finer fibres, fibrils or micro fibrils.
12. A method as claimed in any of claims 4 to 11 wherein energy is
introduced may means including laser etching, ultrasonic, plasma,
mechanical raising or emerising, separately or in combination.
13. A method as claimed in any of claims 4 to 12 wherein the fibres
are keratinous fibres.
14. A method as claimed in claim 13 wherein the fibres are selected
from cashmere, camel, alpaca, mohair, and especially wool.
15. A method as claimed in any of claims 4 to 14 wherein the fibres
are initially scoured using a detergent or surfactant.
16. A method as claimed in any of claims 4 to 15 wherein the
chemical treatments of the first and second steps are applied using
the "exhaustion" technique from long liquors.
17. A method as claimed in any of claims 4 to 16 wherein a reducing
agent is used following step two.
18. A method as claimed in claim 17 wherein the reducing agents is
sodium sulphite or sodium bisulphite.
Description
[0001] This invention relates to a method for fibrillating natural
fibres, and in particular relates to a method for fibrillating
keratinous fibres such as wool and to a fibrillated product.
[0002] Fibrillation refers to the separation of wool fibres into
finer elements, or fibrils, of smaller diameter. These maybe me
macro-fibrils, proto-fibrils, or combinations thereof. Fibrillation
of certain cellulosic fibres has been widely studied, and
fibrillation can be utilised to improve fabric performance, for
example strength, absorbency, surface area together with handle and
opacity. However, it believed that keratinous fibres such as wool
have not been treated in this way.
[0003] The invention seeks to provide a fibrillated keratinous
fibre fabric and a method of fibrillating natural fibres.
[0004] According to the broadest aspect of the present invention
there is provided a textile fabric of keratinous fibres
characterised by the presence of fibrils, micro-fibrils and
proto-fibrils.
[0005] The fibrils may be further characterised as having diameters
in the range 3 .mu.m to 5 .mu.m and by having lengths in the range
25 .mu.m to 60 .mu.m.
[0006] Preferably, the fabric is a woven, knitted, non-woven or
composite fabric.
[0007] The invention also provides a method of treating natural
fibres which comprises:
[0008] a pre-treatment to remove surface lipid materials or
scales;
[0009] a treatment to remove or partially remove intercellular
cement; and
[0010] the application of mechanical agitation under aqueous
conditions to complete fibrillation.
[0011] For preferential control of the fibre fibrillation, a
pre-treatment to remove, modify or change the surface chemistry of
keratin fibres is required.
[0012] The pre-treatment is necessary, with wool fibres, to remove
surface lipid materials or scales which enclose the fibre core.
This may be carried out with an oxidising agent, preferably using
any of the oxidising agents widely known in connection with wool
treatments (e.g. for imparting shrink resistant characteristics)
such as Permonosulphuric Acid or its salt (PMS),
Dichloroisocyanuric Acid or its salt (DCCA), Sodium Hypochlorite,
Gaseous or liquid chlorine, peracetic acid, hydrogen peroxide,
agqueous bromine, or, alternatively, electrical discharge (plasma)
treatments, applied singly or in combination
[0013] The second stage of the process, namely removal of
intercellular cement, may conveniently be carried out using an
enzyme treatment, e.g. Papain, which is of vegetable origin and is
successfully used by industry in other applications. Other
alternatives include, without limitation, Scintillase, Esperase
8.0L, Durazyme 16.0L, Bactosol WO, Pronase, Alcalase, Savinase,
Novozyme 735, Trypsin or Pepsin, separately or in combination.
Reducing agents may be used in the enzyme bath, e.g. Dithionite,
L-cysteine, or thioglycollice acid.
[0014] The mechanical agitation is preferably carried out under
aqueous conditions. Energy may be introduced by the process known
as "hydroentanglement" in which water jets are used to agitate the
fibres and partially break them down into smaller, finer fibres,
fibrils or micro fibrils. Other effective treatments may include
laser etching, ultrasonic, plasma, mechanical raising or emerising.
Mechanical treatments to the fabric may be carried out using either
one method or a combination of such methods.
[0015] The process of the invention is particularly effective with
keratinous fibres, for example wool, which normally cannot be
fibrillated by chemical treatment or mechanical agitation alone. It
has been found that the method of the present invention is
successful in fibrillating keratinous fibres. Although primarily
concerned with keratinous fibres, it has also been found that
excellent results can be obtained when the method of the invention
is applied to other natural fibres such as silk and natural
cellulosic fibres. Although some fibrillation can be achieved
without the process of the invention, particularly with
cellulosics, it has been found that the method produces enhanced
results.
[0016] Keratinous fibres which may be employed in the fabric and
method of the invention include, but are not limited to, cashmere,
camel, alpaca, mohair, and especially wool.
[0017] In order to facilitate the method of the invention, it is
preferable that the fibres are initially scoured using a detergent
or surfactant common in the textile field.
[0018] It is preferred that the chemical treatments of the first
and second steps of the invention are applied using the
"exhaustion" technique from long liquors.
[0019] It is preferred to use a reducing agent following the enzyme
treatment in step 2 of the method. Suitable reducing agents are
those widely known in textile processing such as sodium sulphite or
sodium bisulphite.
[0020] The invention will be described further in the following
examples, which are for illustrative purposes only. Reference is
made to the accompanying drawings, in which:
[0021] FIG. 1 comprises four bar charts of frequency distribution
of fibril diameter; and
[0022] FIG. 2 comprises four bar charts of frequency distribution
of fibril length.
EXAMPLES
[0023] It was observed that fibre fibrillation can be achieved by
treating samples with both chemical and mechanical processes in
sequence. The chemical pre-treatment steps remove the surface lipid
material or scales from the surface of the fibre and then break
down the intercellular cement. The introduction of mechanical
energy in the form of high pressure water jets further breaks down
the intercellular cement resulting in the emergence of macrofibrils
from the cortical cells. Fibrillation is clearly in evidence and
has a marked effect on fabric handle.
[0024] 1. Wool Fibres
[0025] Fibrillation or separation of fibres into finer elements is
achieved by treating samples with both chemical and mechanical
processes in sequence.
[0026] 2. Cashmere
[0027] The fibre is pretreated with the same chemicals as used for
wool. It is then subjected to mechanical energy, preferably
hydroentanglement.
[0028] Examples of the chemical treatments that can be used are
listed in table 1.
[0029] All samples were passed through a hydroentanglement machine
using four injectors each operating at a fabric specific energy
treatment of 100 bar water pressure (3.04 mj/kg).
1TABLE 1 Some Combined chemical and mechanical treatments used to
obtain fibre fibrillation Chemicals Mechanical treatment Treatment
Oxidising agent Enzyme agent Reducing agent Temperature (see table
2) A DCCA (6% owf) Papain (4% owf) +
Na.sub.2SO.sub.3.7H.sub.2o/Na.sub.2S.sub.2O.sub.5 20.degree. C. Yes
(NH.sub.4).sub.2SO.sub.4 10/10(% owf) B PSA (6% owf) Papain (3.5%
owf) Na.sub.2SO.sub.3.7H.sub.2o/Na.sub.2S.sub.2- O.sub.5 20.degree.
C. Yes 10/10(% owf) C DCCA (7% owf) Papain (1.5% owf)
Na.sub.2SO.sub.3.7H.sub.2o/Na.sub.2S.sub.2O.sub.5 20.degree. C. Yes
10/10(% owf) D DCCA (5% owf) Papain (3.0% owf)
Na.sub.2SO.sub.3.7H.sub.2o/Na.sub.2S.sub.2O.sub.5 20.degree. C. Yes
10/10(% owf)
[0030] There is no universally accepted standard method for the
assessment of fibre fibrillation. Taylor (1993) introduced a
Fibrillation Index, which is based on the use of a microscope to
count the individual fibrils on the fibre surface. Obviously, this
is a tedius method and because the fibrillation is not necessarily
evenly distributed across the fabric, randomly selected fibres from
a sample may produce biased results.
[0031] In order to evaluate fibre fibrillation an optical method
was used based on image analysis of SEM images. In this method the
light intensity level along a pixel line within the image is
measured. The variation of light intensity along this line (which
crosses the fibre perpendicular to its axis) can be used to obtain
direct measurements of fibril diameter.
[0032] The results of treatments A-D (Table 1) are shown in FIG. 1.
It was established that using treatment A, 50% of fibrils have a
diameter of about 3 .mu.m and an average fibril diameter of 5
.mu.m. Applying treatment B results in an average fibril diameter
of 4.8 .mu.m whereas, using treatment C a narrower range of fibril
diameters with an average of 3.2 .mu.m was obtained. On the other
hand, treatment D resulted in an apparently normal distribution
with an average diameter of 4.4 .mu.m.
[0033] It should be noted that the skewed shape of some of the
distributions may be due to limitations of the measuring system at
650.times. magnification. At this magnification, finer fibrils
could not be clearly resolved by the microscope, and therefore
measured by image analysis.
[0034] SEM images and image analysis were used to assess the length
of fibrils detached from the parent fibre. The results of these
measurements are shown in FIG. 2. Treatment A resulted in 50% of
fibrils with a length of 45 .mu.m with a skewed distribution. The
average length was 40 .mu.m. The average fibril length obtained
using treatment B was 41 .mu.m. In comparison with the other
treatments a shorter fibril length resulted from treatment C with
an average of 31 .mu.m whereas, treatment D showed a wider range of
fibril lengths with an average length of 51 .mu.m.
[0035] Chemical treatment alone can remove the wool scale structure
but there is no concurrent fibrillation. The introduction of
mechanical treatment alone in the form of high pressure water jets
also resulted in no fibre fibrillation. On the other hand, when
both chemical and mechanical treatments are applied in succession,
significant fibre fibrillation can be obtained.
[0036] While not so-limited, it is believed that the fabric and
method of the invention have two principal uses. Firstly, it may be
used with woven, knitted, non-woven or composite fabrics to give a
soft "fuzzy" fibrous surface or pile. Indeed, a very fine "peach
skin" effect can be obtained. Patterning of the fabric surface
appearance and texture can be achieved by localising the areas
having fibrils, micro-fibrils and/or proto-fibrils, e.g. by
selective application of the chemical treatment.
[0037] It can also be used to make non-woven fabrics. These, owing
to the microfibrils, can be finer and/or denser than before. This
means that less fibres are needed for a particular fabric, or,
where the same number of fibres are employed, a denser fabric can
be produced. One embodiment involves pre-treatment of the fibre
before web formation followed by hydroentanglement, which is used
both to consolidate the web and to split the fibres.
[0038] Consolidation and fibre splitting can be achieved either
concurrently or sequentially in hydroentanglement in regard to
keratinous fibres such as wool.
[0039] The degree of fibre pre-strain (stored strain) resulting
from preparatory processes such as carding can also influence the
degree of fibrillation or splitting of the fibres, when mechanical
energy is subsequently applied. It may be beneficial to increase
fibre strain by tensioning the fabric before or during application
of the mechanical eery (e.g. by use of a fabric stenter machine).
As referred to above, the invention is primarily useful in
connection with keratinous fibres such as wool. It is also
particularly useful with fibres of 21 microns diameter or above,
particularly for coarser wools, such as British or New Zealand
wools, where it produces a substantial beneficial effect.
* * * * *